JPH03138365A - Target member and its production - Google Patents
Target member and its productionInfo
- Publication number
- JPH03138365A JPH03138365A JP27624489A JP27624489A JPH03138365A JP H03138365 A JPH03138365 A JP H03138365A JP 27624489 A JP27624489 A JP 27624489A JP 27624489 A JP27624489 A JP 27624489A JP H03138365 A JPH03138365 A JP H03138365A
- Authority
- JP
- Japan
- Prior art keywords
- target member
- relative density
- powder
- alloy powder
- uniformly distributed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 238000000034 method Methods 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 20
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 13
- 239000000956 alloy Substances 0.000 claims abstract description 13
- 238000007712 rapid solidification Methods 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 5
- 239000002184 metal Substances 0.000 claims abstract description 3
- 229910052751 metal Inorganic materials 0.000 claims abstract description 3
- 239000002245 particle Substances 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims 1
- 239000000203 mixture Substances 0.000 abstract description 9
- 238000009689 gas atomisation Methods 0.000 abstract description 5
- 230000001105 regulatory effect Effects 0.000 abstract 2
- 238000004544 sputter deposition Methods 0.000 description 9
- 238000002844 melting Methods 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- 229910000831 Steel Inorganic materials 0.000 description 5
- 230000005496 eutectics Effects 0.000 description 5
- 239000010959 steel Substances 0.000 description 5
- 238000001513 hot isostatic pressing Methods 0.000 description 4
- 238000005096 rolling process Methods 0.000 description 4
- 239000006104 solid solution Substances 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910001362 Ta alloys Inorganic materials 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000010587 phase diagram Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 229910020676 Co—N Inorganic materials 0.000 description 1
- 229910001208 Crucible steel Inorganic materials 0.000 description 1
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- 229910018487 Ni—Cr Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004453 electron probe microanalysis Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000005098 hot rolling Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000005204 segregation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005477 sputtering target Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、磁気記録用Ｇ ｏ−Ｃｒ−Ｔ ａ磁性膜をス
パッタ法により作成するためのターゲット部材およびそ
の製造法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a target member for creating a Go-Cr-Ta magnetic film for magnetic recording by sputtering, and a method for manufacturing the same.
スパッタ法による磁性膜にＣｏ−ＮＬ Ｃｏ−Ｃｒある
いはＣｏ−Ｎｉ−Ｃｒが従来から工業的に使用されてき
た。そして近年、磁性膜に起因するノイズの低減、スパ
ッタ膜（磁性膜）の高保磁力化の要求により、Ｃｏ−Ｎ
ｉ、Ｃｏ−ＣｒあるいはＣｏ−Ｎｉ−ＯｒにＴａを添加
した合金が磁性膜に使用されるようになり、現在では記
録媒体の主流となっている（特開平１−１３３２１７号
参照）。Co-NL Co-Cr or Co-Ni-Cr has been used industrially for magnetic films formed by sputtering. In recent years, Co-N
An alloy of Co--Cr or Co--Ni-Or with Ta added has come to be used for magnetic films, and is now the mainstream of recording media (see Japanese Patent Laid-Open No. 1-133217).
一方、含有されるＴａ量も、初期へのＴａ＝１原子ｉか
らなる２原子ｉ以上と、高保磁力化のため増加しつつあ
る。On the other hand, the amount of Ta contained is also increasing to 2 atoms i or more consisting of Ta=1 atom i in the initial stage due to the increase in coercive force.
このスパッタ膜形成に使用するターゲット部材は、従来
、溶解・鋳造まま、もしくは熱間や冷間加工して薄板ま
で成形し、それから加工採取されていた。Conventionally, the target member used for forming this sputtered film has been melted or cast as it is, or hot or cold worked to form a thin plate, and then processed and sampled.
Ｃｏ−Ｃｒ−Ｔａ合金の磁性膜を製作するために使用さ
れるスパッタリングターゲット部材の従来の製造法は溶
解・鋳造した鋼塊を加工することによって行なわれてい
た。A conventional method for manufacturing a sputtering target member used for manufacturing a Co--Cr--Ta alloy magnetic film is to process a melted and cast steel ingot.
Ｃｏ−Ｃｒ−Ｔａａ元合金の状態図は未知であるが、Ｃ
ｏ−Ｔａの場合、１２７６℃の共晶温度において、α−
Ｃｏ中へのＴａの固溶度は４〜５ａｔ％である。The phase diagram of the Co-Cr-Taa base alloy is unknown, but C
In the case of o-Ta, at the eutectic temperature of 1276°C, α-
The solid solubility of Ta in Co is 4 to 5 at%.
Ｃｏ−１０／２０Ｃｒ−Ｔａ合金においても、基地はＣ
ｏ−１０７２０Ｃｒから構成されているとみなすと、Ｔ
ａは４〜５ａｔ％固溶すると考えられる。Even in Co-10/20Cr-Ta alloy, the base is C
Considering that it is composed of o-10720Cr, T
It is thought that a is dissolved in solid solution at 4 to 5 at%.
しかし、工業的な溶解・鋳造においては、平衡状態図か
らのズレを生じる。現象的には鋳型に接して最初に凝固
する鋼塊の外周部はＴａが固溶された組織を示すが、最
終凝固に近い部分はＴａが合金全体の平均値より富化し
、共晶温度でＬｉｑ→α−Ｃｏ＋Ｃｏ、Ｔａの共晶反応
を生じる。すなわち、鋼塊の中心部はＴａ富化のＣｏ１
Ｔａがミクロ的に偏析する。このような鋼塊を熱間加工
で薄板化したターゲット部材は、厚さ方向にＴａ１ｌが
異なる不均質なターゲット部材となる。このような不均
質なターゲット部材を用いて得られたスパッタ膜の組成
は、スパッタリングの経通に伴い変化し、磁気特性の変
化を生じさせるという問題があった。However, in industrial melting and casting, deviations from the equilibrium phase diagram occur. In terms of phenomena, the outer periphery of the steel ingot that first solidifies in contact with the mold shows a structure in which Ta is dissolved as a solid solution, but in the part near the final solidification, Ta is enriched more than the average value of the entire alloy, and Ta is enriched at the eutectic temperature. A eutectic reaction of Liq→α-Co+Co and Ta occurs. In other words, the center of the steel ingot is Ta-enriched Co1.
Ta is microscopically segregated. A target member obtained by thinning such a steel ingot by hot working becomes a non-uniform target member with Ta1l varying in the thickness direction. The composition of a sputtered film obtained using such a non-uniform target member changes with the course of sputtering, causing a problem in that the magnetic properties change.
本発明の目的は、スパッタリングの最初からターゲット
部材の寿命まで特性の変化しないスパッタ膜を生成する
ターゲット部材およびその製造方法を提供するものであ
る。An object of the present invention is to provide a target member that produces a sputtered film whose characteristics do not change from the beginning of sputtering to the life of the target member, and a method for manufacturing the same.
本発明は、原子％でＣｒ８〜１８％、Ｔａ２〜８％、残
部実質的にＣｏよりなり、Ｔａが均一に分布しかつ相対
密度が９８％以上である焼結体であることを特徴とする
ターゲット部材、およびそのターゲット部材の製造方法
であって、原子％でＣｒ８〜１８％、Ｔａ２〜８％、残
部実質的にＣｏよりなる粒径３２メツシュ以下の急冷凝
固法により製造された合金粉末を金属製容器に充填封入
した後、加圧焼結することを特徴とするターゲット部材
の製造方法である。The present invention is characterized by a sintered body consisting of 8 to 18% Cr, 2 to 8% Ta, and the remainder substantially Co, in which Ta is uniformly distributed and the relative density is 98% or more. A target member and a method for manufacturing the target member, comprising an alloy powder manufactured by a rapid solidification method with a particle size of 32 mesh or less consisting of 8 to 18% Cr, 2 to 8% Ta, and the remainder substantially Co in atomic %. This method of manufacturing a target member is characterized in that the target member is filled and sealed in a metal container and then sintered under pressure.
以下、本発明の詳細な説明する。The present invention will be explained in detail below.
本発明の特徴は、ガスアトマイズ法等の急冷凝固法によ
り製造した所定組成の合金粉末を用いることにある。す
なわち、この粉末は凝固に対する冷却速度が大きいため
、Ｔａを均一に固溶もしくは一部Ｃｏ、Ｔａを晶出した
組織を有するため、これを用いて得られるターゲット部
材は、ターゲット部材の表面、板厚中央部とも従来の溶
解・鋳造法によるものと異なり、Ｔａが均一に分布した
組成を示す。A feature of the present invention is the use of alloy powder of a predetermined composition produced by a rapid solidification method such as a gas atomization method. That is, since this powder has a high cooling rate for solidification, it has a structure in which Ta is uniformly dissolved in solid solution or in which Co and Ta are partially crystallized. Both the thick central part exhibits a composition in which Ta is uniformly distributed, unlike that obtained by conventional melting and casting methods.
急冷凝固法としては、前述のガスアトマイズ法の他に真
空アトマイズ法、回転ロール法、回転電極法等の公知の
粉末製造法が適用できる。回転ロール法、回転電極法等
においても合金の酸化防止のために、雰囲気は真空、不
活性ガス雰囲気とするのが望ましい、なお、急冷凝固法
のなかでは高いタップ密度が得られる球状粉を形成しや
すく、かつ生産コストの有利なガスアトマイズ法が望ま
しい。As the rapid solidification method, in addition to the above-mentioned gas atomization method, known powder manufacturing methods such as a vacuum atomization method, a rotating roll method, and a rotating electrode method can be applied. In the rotating roll method, rotating electrode method, etc., it is preferable to use a vacuum or inert gas atmosphere in order to prevent oxidation of the alloy.In addition, among the rapid solidification methods, spherical powder with a high tap density is formed. A gas atomization method is desirable because it is easy to perform and has an advantageous production cost.
以上の急冷凝固法により得られた合金粉末のうち、粒度
が３２メツシュ以下のものを用いる。Among the alloy powders obtained by the above rapid solidification method, those having a particle size of 32 mesh or less are used.
このように粉末の粒度を３２メツシュ以下としたのは、
焼結時過飽和固溶体から析出するｃｏ、Ｔａ分布の均質
性が劣ってくるためである。In this way, the particle size of the powder was set to 32 mesh or less because
This is because the homogeneity of the distribution of Co and Ta precipitated from the supersaturated solid solution during sintering becomes poor.
ついで、この合金粉末を加圧焼結し、相対密度が９８％
以上の焼結体を得る。This alloy powder is then pressure sintered to a relative density of 98%.
The above sintered body is obtained.
相対密度を９８％以上とするのは、これ未満の密度で気
泡が存在するとスパッタ作業中異常放電を起こすためで
ある。The reason why the relative density is set to 98% or more is because the presence of bubbles at a density lower than this causes abnormal discharge during sputtering work.
加圧焼結の方法としては、熱間静水圧プレス（ＨＩＰ）
、ホットプレス、熱間パック圧延、鍛造等が適用できる
が、９８％以上の高密度を得るためにはＨＩＰが最も望
ましい。Hot isostatic pressing (HIP) is a method of pressure sintering.
, hot pressing, hot pack rolling, forging, etc. can be applied, but HIP is most desirable in order to obtain a high density of 98% or more.
このＨＩＰは、温度１０００−１２５０℃、圧力５００
ａｔ＋ｓ以上の条件で実施される必要がある。ここで温
度の上限を１２５０℃としたのはＣｏ−Ｔ ａの共晶温
度が１２７６℃であり、粉末内でミクロ的にＴａ豊化の
部分に融液が生じるためである。一方、温度の下限を１
０００℃としたのは１、これ未満では焼結密度が９８％
以上に上らないためである。This HIP is performed at a temperature of 1000-1250℃ and a pressure of 500℃.
It is necessary to carry out the test under conditions of at+s or higher. The reason why the upper limit of the temperature is set to 1250°C is that the eutectic temperature of Co-Ta is 1276°C, and a melt is generated in microscopically Ta-enriched parts of the powder. On the other hand, set the lower limit of temperature to 1
000℃ is 1, below this the sintered density is 98%
This is to prevent it from rising above that level.
また、圧力を５００ａｔｍ以上とするのは、やはりこれ
未満では、焼結体の相対密度を９８％以上にすることが
困難だからである。Further, the reason why the pressure is set to 500 atm or more is that if the pressure is less than this, it is difficult to make the relative density of the sintered body 98% or more.
また熱間静水圧プレス等による加圧焼結に続いて熱間加
工を行なうと、相対密度が向上し、よりスパッタ特性の
安定したターゲット部材が得られる。Further, when hot working is performed subsequent to pressure sintering using hot isostatic pressing or the like, the relative density is improved and a target member with more stable sputtering characteristics can be obtained.
本発明のターゲット部材は、ａｔ％でＣｒ８〜１８％、
Ｔａ２〜８％、残部実質的にＣｏからなる組成を有する
が、これは特開平１−１３３２１７号に開示されるよう
この範囲で保磁力がＨｅ≧６００ （Ｏｅ）の値が得ら
れ、膜のノイズレベルも小さくて、磁気記録媒体として
優れた特性を示すからである。特にＴａは２ａｔ％末滴
では通常の溶解法で鋼塊中のＴａの偏析が少な（，８ａ
ｔ％を越えると飽和磁化が１０００［Ｇ］未満と小さく
なりすぎて、磁気記録に適さなくなるため、Ｔａを２〜
８ａｔ％に限定した。The target member of the present invention has Cr8 to 18% in at%,
It has a composition consisting of 2 to 8% Ta and the remainder substantially Co. As disclosed in JP-A-1-133217, a coercive force of He≧600 (Oe) can be obtained in this range, and the film is This is because the noise level is low and exhibits excellent characteristics as a magnetic recording medium. In particular, when Ta is used as a 2at% powder drop, there is little segregation of Ta in the steel ingot using the normal melting method (, 8a
If it exceeds t%, the saturation magnetization becomes too small, less than 1000 [G], making it unsuitable for magnetic recording.
It was limited to 8 at%.
以下、本発明を実施例に基づき説明する。 The present invention will be explained below based on examples.
原子％で１２Ｃｒ−３Ｔａ−残部Ｃｏ組成の合金粉末を
ガスアトマイズで製作した。続いて、この粉末を分級し
３２メツシュ以下の粉末を７ｋｇ秤量した。An alloy powder having a composition of 12Cr-3Ta-balance Co in atomic % was produced by gas atomization. Subsequently, this powder was classified and 7 kg of powder having a size of 32 mesh or less was weighed.
この粉末を軟鋼製の缶に充填し、脱気、封止したのち熱
間静水圧プレスで１１００℃、 １０００ａｔ−で焼結
を行なった０次に、この箱体を熱間圧延により厚さ８−
に仕上げ、両側の鉄皮をはいで６Ｍの板材を採取した。This powder was filled into a mild steel can, degassed and sealed, and then sintered in a hot isostatic press at 1,100°C and 1,000 at.Next, the box was hot rolled to a thickness of 8. −
The iron skin on both sides was removed and 6M plates were collected.
一方、原子％で１２ｃｒ−３Ｔａ−残部Ｃｏ組成の合金
を真空溶解したのち３０ｋｇ鋼塊を製造し、ハンマー分
塊と熱間圧延により６ＩＩＩＩｌｌの板材を作製した。On the other hand, a 30 kg steel ingot was produced by vacuum melting an alloy having a composition of 12cr-3Ta-balance Co in atomic %, and a 6IIIll plate material was produced by hammer blooming and hot rolling.
次に粉末および溶解法で製造した板材より、５ｔｘ１０
２φのターゲット部材を採取した。このターゲット部材
を使用して、軟質ガラス上に純Ｃｒ下地膜を０．１μＩ
成膜した上に、高周波出力３００−１Ａｒ操作圧力３Ｘ
１０°３ｔｏｒｒの条件下で５００人成膜し、振動磁力
計で膜の保磁力を測定した。Next, from powder and plate materials manufactured by melting method, 5tx10
A 2φ target member was collected. Using this target member, a pure Cr underlayer film was deposited at a thickness of 0.1μI on soft glass.
In addition to film formation, high frequency output 300-1Ar operating pressure 3X
A film was formed by 500 people under conditions of 10° and 3 torr, and the coercive force of the film was measured using a vibrating magnetometer.
第１表にターゲット部材表面層と中心部のＥＰＭＡによ
る組成の分析値（ａｔ％）とターゲット部材のその位置
に対応するスパッタ膜の磁性値を示す。Table 1 shows the EPMA composition analysis values (at%) of the surface layer and center of the target member and the magnetic values of the sputtered film corresponding to those positions on the target member.
第１表かられかるように粉末法で作製したターゲット部
材は表面および板厚中心で組成に変動がなく、スパッリ
ングにより成膜した膜の磁性値もほとんど変動が認めら
れない。As can be seen from Table 1, there is no change in the composition of the target member produced by the powder method on the surface and at the center of the plate thickness, and almost no change is observed in the magnetic value of the film formed by sputtering.
一方、従来法で製造したターゲット部材は表面層は平均
値より若干Ｔａは少なく、板厚中心部は共晶により生じ
たＣｏ、Ｔａが熱間加工により圧延方向に線状に伸びた
部分が存在し、Ｔａ量が高くなっている。また、スパッ
タ膜の保磁力もターゲット部材表面と板厚中心部で値が
異なることが知られた。On the other hand, in the target member manufactured by the conventional method, the surface layer has slightly less Ta than the average value, and in the center of the plate thickness there is a part where Co and Ta produced by eutectic elongate linearly in the rolling direction due to hot working. However, the amount of Ta is high. It has also been found that the coercive force of the sputtered film is different between the surface of the target member and the center of the plate thickness.
よる本発明のターゲット部材およびその製造方法は、工
業上顕著な効果を有するものである。The target member and the method for manufacturing the same of the present invention have significant industrial effects.
第１表、 桁値とスパッタ の 磁力〔発明の効果〕
以上説明したように、Ｃｒ ８／ １８− Ｔ ａ２／
８−残部にＯターゲット部材を粉末法で作製した場合、
従来の溶製法で作製したターゲット部材に比較して、タ
ーゲット部材内部での組成変動が少なく、スパッタ時の
経過に伴う生成膜の磁性値変動も小さい結果が得られた
。Table 1, Digit value and sputtering magnetic force [Effect of the invention] As explained above, Cr 8/ 18-Ta2/
8- If the O target member is made in the remaining part by the powder method,
Compared to target members produced by conventional melting methods, results were obtained in which compositional fluctuations within the target member were small and magnetic value fluctuations of the produced film over time during sputtering were also small.
Claims (1)
的にＣｏよりなり、Ｔａが均一に分布しかつ相対密度が
９８％以上である焼結体であることを特徴とするターゲ
ット部材。 ２ 請求項１記載のターゲット部材の製造方法であって
、原子％でＣｒ８〜１８％、Ｔａ２〜８％，残部実質的
にＣｏよりなる粒径３２メッシュ以下の急冷凝固法によ
り製造された合金粉末を金属製容器に充填封入した後、
加圧焼結することを特徴とするターゲット部材の製造方
法。[Claims] A sintered body consisting of 1 atomic % of 8 to 18% Cr, 2 to 8% Ta, and the remainder substantially Co, in which Ta is uniformly distributed and the relative density is 98% or more. Characteristic target parts. 2. The method for producing a target member according to claim 1, wherein the alloy powder is produced by a rapid solidification method and has a particle size of 32 mesh or less and consists essentially of 8 to 18% Cr, 2 to 8% Ta, and the remainder Co in terms of atomic %. After filling and sealing in a metal container,
A method for manufacturing a target member, characterized by performing pressure sintering.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27624489A JP2909108B2 (en) | 1989-10-24 | 1989-10-24 | Target member and method of manufacturing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP27624489A JP2909108B2 (en) | 1989-10-24 | 1989-10-24 | Target member and method of manufacturing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03138365A true JPH03138365A (en) | 1991-06-12 |
| JP2909108B2 JP2909108B2 (en) | 1999-06-23 |
Family
ID=17566712
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP27624489A Expired - Fee Related JP2909108B2 (en) | 1989-10-24 | 1989-10-24 | Target member and method of manufacturing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2909108B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001077403A1 (en) * | 2000-04-07 | 2001-10-18 | Unaxis Materials Ag | Metal or metal alloy based sputter target and method for the production thereof |
| JP2009221608A (en) * | 2009-07-07 | 2009-10-01 | Mitsui Mining & Smelting Co Ltd | Sputtering target |
| JP2009263796A (en) * | 2003-08-05 | 2009-11-12 | Nippon Mining & Metals Co Ltd | Sputtering target and method for production thereof |
-
1989
- 1989-10-24 JP JP27624489A patent/JP2909108B2/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001077403A1 (en) * | 2000-04-07 | 2001-10-18 | Unaxis Materials Ag | Metal or metal alloy based sputter target and method for the production thereof |
| JP2009263796A (en) * | 2003-08-05 | 2009-11-12 | Nippon Mining & Metals Co Ltd | Sputtering target and method for production thereof |
| JP2009221608A (en) * | 2009-07-07 | 2009-10-01 | Mitsui Mining & Smelting Co Ltd | Sputtering target |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2909108B2 (en) | 1999-06-23 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |